Method of treating cellulose organic derivative cut staple fibers



Patented Apr. a, 1940 .METHOD or TREATING oELLULosE on GANIC DERIVATIVE.curv STAPLE mans Wallace T. Jackson and Wendell G. Faw, Kingsport,Tenn., assignors to Eastman Kodak Company, Rochester, N. Y.

Jersey No Drawing at corporation of New Application December 3, 1936,-Serial No.-114 ,077

9 claims. (01. 19-66) This invention relates to the manufacture ofcellulose organic derivative cut staple fibers, and more particularly toa method of eliminating the tendency of such fibers to accumulatecharges of 5 static electricity in the various steps involved in themanufacture therefrom of spun yarns and fabrics.

As is well-known, cellulose organic derivative materials, particularlyin filament, yarn, or sheet 10 form, are particularly subject to theaccumulation on their surfaces of charges of static electricity fromfrictional influences. In the case of filaments and yarns in which thesurface area of the material (per unit of weight) is enormously 15greater as compared to sheets or films, the problem of static oftenassumes serious proportions. In the manufacture of yarns of varioustypes from artificial filaments, numerous steps in which the yarn issubjected to frictional influences may be a necessary, as for example,twisting, winding, warping, carding, combing, drawing, spinning and thelike, all of which operations tend to produce large accumulations ofstatic on the material. This is particularly aggravated in theutilization u of cut staple, as for example, in the making of spun yarn,since in carding and combing considerable friction is developed and as aresult sumcient static accumulates on the fibers to make the formationof the web difiicult, if not imposao sible; furthermore, even if a webis formed with some degree of success, the subsequent drafting operationproduces a very uneven spun yarn or intermediate roving, due to thepresence of. the static charge. In addition, there is the evera presentfire hazard.

Cellulose derivative yarnyparticularly in the form of cut staple, isextremely difiicult to handle in the various operations involved inmaking spun yarn, not only because such material is composed a offilaments having smooth, glassiike, surfaces without natural kink orirregularity, but also because it has relatively negligible moisturecontent at normal humidities. These characteristics of this type of yarncause it to be inherently more a susceptible to accumulation ofstaticcharges than natural fibers such as cotton and wool. Indeed,

the charges accumulating on cellulose derivative staple fibers are,under some circumstances, suflicient to separate the individualfibers adistance of inches, notwithstanding their relatively small size.

This inventionv has as its principal object to provide an improvedmethod for the manufacture of cellulose organic derivative cut staplefibers.

A further object is to provide a method for treating such fibers inwhich the tendency toward accumulation thereon of charges of staticelectricity is reduced or eliminated. A still further object is toprovide a method of facilitating the handling and employment ofcellulose organic derivative cut staple fibers in the various operationsinvolved in the manufacture of spun yarns, wherein the staple issimultaneously softened and lubricated and the accumulation of staticcharges thereon is prevented. Another object is to provide an improvedtype of cellulose organic derivative cut staple having little or notendency toward accumulation of static electrical charges. Other objectswill appear hereinafter.

These objects are accomplished by the following invention which, in itsbroader aspects, comprises applying to cellulose organic derivative cutstaple of setyl alcohol having the following formula A specific exampleof a composition containing this and other similar amine salts which wehave found valuable for our purpose is one composed of about 22-45% byweight of the diethyl cyclohexylamine salts of sulphated decyl, lauryl,cetyl and'myricyl alcohols, the balance being chieflya 40 lubricant orconditioning agent such. as mineral ,-oil. This composition may containvarying proportions of similar amine salts of several different higheraliphatic alcohols. a i

The broad scope of our invention also includes the application tocellulose organic derivative cut staple fibers of other antistaticagents as, for. example, salts formed by interaction of an organic .basesuch as an alkyl amine, a substituted alkyl amine, an alicyclicamine oran alkylolamine, with an aromatic sulfonic acid. Examples of suchorganic bases are amylamine, diamyl amine, cyclohexylamine andtriethanolamine. The aromatic slilfonic acid may contain a singlearomatic nucleus, as in the case of benzenesulfonic acid, 5

or it may be of the fused or polynuclear type as represented by thenaphthalene sulfonic acids. The acids may be monoor polysulfonic acids,and may contain other substituents in the nucleus,

such as alkyl, amino, hydroxyl and other groups,

. typical'examples of these acids being paratoluene sulfonic acid,orthoaminobenzene sulfonic acid, 2-naphthol-6-sulfonic acid, and isomersthereof. Specific examples of this, type ofsalt are triethanolaminebenzenesulfonate, amylamine paratoluene sulfonate, and triethanolaminetoluene sulfonate. Examples of the compounded antistatic oil itselfwhich have been found, in accordance with our invention, to give highly'satisfac tory results as antistatic agents when applied in the form ofaqueous emulsions to cellulose organic derivative cut staple fibers arethe following:

The broad scope of this invention also includes the application tocellulose organic derivative cut staple fibers of additional antistaticagents as for example-salts formed by interaction of an organic base,such as those above mentioned, as well as amines containing an etherlinkage, with an organic acid containing a cyclic ether residue'or I soan organic acid containing an open chain ether residue. Morespecifically, such salts may be formed by reacting an acid containing anether linkage, such as tetrahydrofuroic acid with a base (amine)containing an ether linkage, giving. such as tetrahydrofurfuryl amine,tetrahydrofurfurylamine tetrahydrofuroate; an acid containing no etherlinkage such as butyric acid with an amine containing an ether linkage,such as tetrahydrofurfuryl amine, giving tetrahydrofurfurylaminebutyrate; an amine containing no ether linkage and preferably six ormore carbon atoms, such as cyclohexylamine, with an acid containing anether linkage, giving such as tetrahydrofuroic acid cyclohexylaminetetrahydrofuroate; an acid containing an unsaturated ether linkage suchas furoic acid with an amine containing a saturated ether linkage, suchas tetrahydrofurfuryl amine giving tetrahydrofurfurylamine furoate. Theuse of this specific class of amine salts just referred to as antistaticagents in the manufacture of cellulose organic derivative cut staple,although included in the broad scope of our invention, is neverthelessthe specific invention of,

and covered by an application in the name of,

J. R. Caldwell, Ser. No. 114,085, filed of even date. We have found thatby applying an amine salt of one of the types described above,preferably mixed or associated with a mineral or vegetable oil, in theform of a solution or an aqueous emulsion of a textile lubricant, tocellulose organic derivative cutstaple fibers, the treated fibers lostsubstantially all tendency to accumulate charges of static electricityand the individual til the advent of the present invention. Ourdiscovery of the antistatic efiect on cellulose derivative cut staple ofthe class of compounds above referred to is especially remarkable inview of the fact that mineral oils, butyl stearate, and

ency to accumulate static charges sufiiciently to make it possible toemploy them in the manufacture of spun yarn.

Our invention may be conveniently described by reference to themanufacture of three different types of cut staple .intended,respectively, for use in the manufacture of spun yarn on the cotton,woolen and worsted systems.

'Emmple I.Referring now to the manufacmm of cellulose organic derivativecut staple for use on the cotton system, the filaments are spun in theusual manner. cellulose acetate spinning dope is extruded in the form ofthree denier filaments through a' spin neret mounted in aconventionaltype of spinning cabinet, the filaments emerging from the cabinet inacompletely cured condition. The filaments are then wound in the form ofa thread on bobbins by means of a cap or ring spinner which imparts tothe thread .a low twist, of .the order of one-half turn per inch.Preferably, the yarn is lubricated tofacilitate twisting and windingasit emerges from the cabinet by the application thereto of a suitabletextile lubricating composition such as an aqueous emulsion of a mineraloil. Yarns from a plurality of bobbins are warped to .a roving ofconvenient size which is fed to a stapling machine, where it is wet withwater and cut to a staple length of to 1 /2 inches. The cut staple isthen scoured to remove the lubricant and placed in a bath of boilingwater and boiled for a period of about 5 minutes. The boiling waterproduces a permanent crimp or kinkiness in the individual fibers. Thecrimped staple is then removed from the boiling bath and treated with anantistatic ,agent of the type mentioned above, such as by immersion, theamount deposited being' equal to about .5-5.%, based onthe dry weight ofthe yarn. The antistatic agent is conveniently applied in the form of anaqueous emulsion at a temperature of about" 0. Following application ofthe no tendency to accumulate electrical charges and unlike ordinaryuntreated staples, are well adapted'for processing in the manufacture ofspun yarns on the cotton. system.

Example II.In the manufacture of cellulose organic derivativecut staplefor use on the worsted system a slightly modified technique is employed'. Inasmuch as natural wool fibers employed in making worstedgoods haverelatively great length (several inches) the cellulosederivative filaments are accordingly cut fairly long. preferably 4 to '7inches.

The filaments as they emerge from the spinning cabinets are wound in theform of cheeses in such manner that they lie in-parallel rela''tionship' to one another. Preferably, andin order to facilitate winding,the filaments are lubricated asthey emerge from the spinning agent in oron the fibers they have substantially r cabinet with a lubricant whichmay, if desired, have antistatic properties. Strands or filaments from aplurality of yarn packages are warped where the filaments are wet cut aspreviously described. The cut staples are then boiled for a period ofabout minutes to crimp them and to give them the characteristicwoollyform. The crimped staple isthen treated with an aqueous emulsion orsolution of one of the agent's above described at a. temperature ofabout 60 0., dried,

and picked. The resulting product is a white woolly appearing mass offibers well adapted for use in the manufacture of {spun yarn on theworsted system.

Example III.Cellulose organic derivative cut staple fibers for use inthe manufacture of spun yarns on the wool system may also be prepared in'a somewhat similarmanner. Such staples are cut to a length ofpreferably 3 to 4 inches, as described in connection with themanufacture of the worsted type staple, dried, picked andthen soaked inan aqueous bath containing a solvent, semi-solvent, or non-solvent ofthe cellulose or-v ganic derivative material of which the fibers arecomposed to bring about the desired crimp. The crimped material is thenpreferably treated with an emulsion or solution of one of the antistaticagents above described and again dried and picked. The resultingmaterial is a soft, white, resilient mass of fibers closely resemblingnatural wool and well-adapted for the manufacture of spun yarns on thewoolen system.

' While we have found it convenient to illustrate our invention byreference to the application ofthe hereindescribed antistaticcompositions ,to

cellulose acetate filaments, threads or cut staple fibers, our inventionis broadly applicable to the treatment of yarns composed of a widevariety of cellulose organic derivatives such as cellulose propionate,cellulose butyrate, cellulose acetate propionate, cellulose acetatebutyrate and other single or mixed organic acid esters of cellulose, aswell as the cellulose ethers.

In general, we prefer to apply relatively small amounts of theantistatic composition to the yarn. In most cases, {g to 5%, based onthe dry weight of the yarn gives excellent results but in some cases wemay use as little as 0.1% or as much as 25% or more.

The most outstanding feature of the agents herein described is theirmarked ability to reduce or eliminate the tendency for cellulosederivative materials to. build up static charges under frictionalinfluences. In determining the peculiar antistatic properties of theseagents, we have made a number of tests particularly designed to measurethe amount of static accumulating on the yarn under different frictionalconditions. In these tests, the yarn was treated, respectively, withbutyl stearate, mineral oil, and an antistatic agent. The treated yarnwas passed first over a steel guide and then over-a porcelain guide atvarious linear speeds and the friction and static charges measured. Inthe case of the yarn treated with butyl stearate it was found that inpassing over each guide the In the case of yarn treated with mineral oilit was found that heavy charges of positive static products.

were developed. In striking contrast to these results, yarn treated withthe antistatic. agents herein described developed no detectable staticcharges whatever. when passingxover the guides under=identicalconditions. In fact no detectable static charges were developedregardless of speed or friction.

As willbe apparent from the above examples and description, theantistatic agents applied' to the yarn in accordance with our inventionremains thereon during the processing of the yarn in the manufacture ofspun yarn and similar It will thus be seen that we have'in realityproduced a new and useful product namely, a cellulose organic derivativecut staple yarn which, unlike untreated yarn, is well adapted forprocessing on'the cotton, woolen or worsted systems. The agents hereindescribed are, however, susceptible of ready removal by means of theordinary scour baths customarily employed in the textile industry.

Our invention has made possible a result not over natural products suchas cotton and wool,

This is an impor but the textile products produced therefrom arecharacterized by properties not attainable in materials obtained fromnatural sources. One of the most outstanding of these properties is thatnatural brilliance or luster peculiar to cellulose derivative materials,ordinarily lacking in natural products.

' While we have chosen to illustrate our inven-- tion by reference tocertain specific antistatic agents, our process is in no sense limitedthereto. On the contrary, the broad scope of our invention includes theapplication to cellulose organic Patent of the United States is:

1. Method of eliminating thetendency of celluloseorganic derivative cutstaple yarns to accumulate charges of static electricity, whichcomprises applying thereto an antistatic composition, the essentialantistatic component of which is a cyclohexyldialkylamine salt of asulphated aliphatic alcohol containing at least 10 lulose organicderivative cut staple yarns to accumulate charges of static electricity,which comprises applying thereto, an antistatic composition, theessential antistatic component of which is a cyclohexyldiethylamine saltof a sulphatedaliphatic alcohol containing at least 10 carbon atoms.

position, an antistatic component of which is a diethylcyclohexylaminesalt of sulphated lauryl alcohol. V

4. Method of eliminating the tendency of cellulose organic derivativecut staple yarns to accumulate charges of static electricity, whichcomprises applying thereto an antistatic composition, an antistaticcomponent of which is a diethylcyclohexylamine salt of sulphated cetylalcohol. 4

5. Method of eliminating the tendency of cellulose organic derivativecut staple yarns to accumulate charges of static electricity, whichcomprises applying thereto an antistatic composition, the essentialantistatic component of which is a mixture of the'diethylcyclohexylamine salts of sulphated decyl, lauryl, cetyl andmyricyl alcohols.' I

6. Method of eliminating 'the tendency of cellulose organic derivativecut staple yarns to accumulate charges of static electricity, whichcomprises applying thereto an antistatic composition composed of about22% to 45% by weight of a mixture of the diethylcyclohexy'lamine saltsof sulphated decyl, lauryl and cetyl alcohols, and 78% to 55% by weightof mineral oil.

7. A cellulose organic derivative out staple yarn containing anantistatic composition, the essential antistatic component of whichcomprises a mixture of the diethylcyclohexylamine salts of decyl,lauryl, cetyl and myricyl alcohols.

8. The method of eliminating the tendency of cellulose organicderivative cut staple yarns to accumulate charges of static electricity,which comprises applying thereto an antistatic com--

